Methyl iodide → HCID 66864160, 화합물

HRID 2093095

반응식

HRID 2093095 반응식
[NH:1]1[C:9]2[CH2:8][CH2:7][N:6]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH2:5][C:4]=2[CH:3]=[C:2]1[C:17]([O:19][CH2:20][CH3:21])=[O:18].[H-].[Na+].[CH3:24]I>C1COCC1>[CH3:24][N:1]1[C:9]2[CH2:8][CH2:7][N:6]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH2:5][C:4]=2[CH:3]=[C:2]1[C:17]([O:19][CH2:20][CH3:21])=[O:18]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 668643095-Tert-butyl 2-ethyl 6,7-dihydro-1H-pyrrolo[3,2-C]pyridine-2,5(4H)-dicarboxylate

생성물 1

HCID 66864160HCID 66864160, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 5-tert-butyl 2-ethyl 1,4,6,7-tetrahydro-5H-pyrrolo[3,2-c]pyridine-2,5-dicarboxylate (1.0 eq) in THF at 0° C. was added NaH (1.2 eq) and stirred for half an hour at room temperature. Methyl iodide (1.3 eq) was added and resulting reaction mixture was stirred for 3 hrs. Reaction mixture was then quenched with water and extracted with ethyl acetate, dried over sodium sulphate and concentrated to dryness. Crude mass was then purified by silica gel column chromatography to afford 5-tert-butyl 2-ethyl 1-methyl-1,4,6,7-tetrahydro-5H-pyrrolo[3,2-c]pyridine-2,5-dicarboxylate.

후처리

  1. customresulting
  2. customreaction mixture
  3. stirringwas stirred for 3 hrs
  4. customReaction mixture
  5. customwas then quenched with water
  6. extractionextracted with ethyl acetate
  7. dry with materialdried over sodium sulphate
  8. concentrationconcentrated to dryness
  9. customCrude mass was then purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-bd144e7436764823bf42c0c4d1686669
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08440830B2

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